CN103450712A - Illite-based composite titanium dioxide and preparation method thereof - Google Patents
Illite-based composite titanium dioxide and preparation method thereof Download PDFInfo
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- CN103450712A CN103450712A CN2013103679132A CN201310367913A CN103450712A CN 103450712 A CN103450712 A CN 103450712A CN 2013103679132 A CN2013103679132 A CN 2013103679132A CN 201310367913 A CN201310367913 A CN 201310367913A CN 103450712 A CN103450712 A CN 103450712A
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Abstract
The invention provides illite-based composite titanium dioxide and a preparation method thereof. The composite titanium dioxide is obtained by coating the surface of illite with nano titanium dioxide particles, and is prepared from the following components in parts by weight: 60-80 parts of illite, 15-35 parts of titanium dioxide and 0.5-5 parts of dispersing agents. The preparation method comprises the steps of depositing, washing and filtering and calcining. The prepared composite titanium dioxide has the characteristics of low cost, high whiteness, strong covering power, low oil absorption and low water-soluble salt value.
Description
Technical field
The present invention relates to a kind of composite titanium dioxide and preparation method thereof.
Background technology
Titanium dioxide (TiO
2), English name Titanium dioxide, be a kind of important Inorganic Chemicals, nontoxic, harmless to health.Be referred to as titanium white (Titanium dioxide white pigment, Titanium white) when titanium dioxide during as white pigment, titanium white is most important white pigment, accounts for 80% of whole white pigment usage quantitys.Titanium resource 90% for the production of titanium dioxide, all the other 10% produce metal titaniums, titanium alloy and pottery etc.Titanium dioxide has become one of three kinds of commodity of sales volume maximum in world's inorganic chemical product, is only second to synthetic ammonia and phosphoric acid.TiO
2there is high opaqueness and good optical property, pigment property as white pigment.Therefore be widely used in the industries such as coating, printing ink, plastics, rubber, papermaking, chemical fibre and daily cosmetics.
The industrial process of titanium dioxide comprises sulfuric acid process and chlorination process at present, accounts for respectively 47% and 53% of global titanium white production, in China, enterprise's employing sulfuric acid process of 95% is approximately arranged.Sulfuric acid process be take ilmenite as raw material, adopts 85% sulfuric acid to be decomposed, and makes titanium compound in ore deposit be transformed into titanium liquid, and the hydrolysis after purifying of titanium liquid is transformed into hydrated titanium dioxide, then obtains the titanium dioxide finished product through washing, calcining and aftertreatment.The sulfuric acid process complexity, long flow path, produce a large amount of spent acid, acid waste water and waste residue in production process, and environmental pollution is extremely serious.Chlorination process is that titaniferous ore (or artificial rutile) is made to titanium tetrachloride through high-temp chlorination, and titanium tetrachloride is at high temperature oxidation generation titanium dioxide and chlorine after purifying again, and the chlorine of generation returns to titanium chloride material.Technical process is short, and automatization level is high, and product specification is high.But, in the chloride process titanium dioxide production process, produce containing radioactive substance and poisonous muriatic waste residue, be difficult to administer and utilize, pollution hazard is very big.Along with continuing to increase of the day by day in short supply and national environmental protection dynamics of Mineral Resources in China, production cost and environmental problem have become the bottleneck of restriction titanium powder industry in China development.
The pigment performance of titanium dioxide particle mainly embodies by optical property, and optical property depends primarily on TiO
2the surface properties of particle, therefore, TiO
2check almost not contribution of optical property in particle.If can use a kind of white material cheap and easy to get to replace TiO
2the particle kernel, the titanium dioxide cost will reduce greatly.
Composite titanium dioxide by adopting cheap mineral as kernel, coats one deck TiO on its surface just
2particle and making.Each state is all at research and exploration composite titanium dioxide, to reduce its cost at present.
Application number is 02135086.8, and denomination of invention is " nanometer CaCO
3/ TiO
2composite particles and preparation method thereof " Chinese patent application, disclose employing Ti (OH) 4 colloidal solution and be deposited on nanometer CaCO
3preparation nanometer CaCO on particle
3/ TiO
2the method of composite particles, but the method goes out Ti (OH) because needs are previously prepared
4colloid, make complex process, and cost is higher, simultaneously the TiO of deposition
2very limited, make the composite particles pigment performance poor.
Application number is 200510080497.3, the Chinese patent application that denomination of invention is " white mineral powder-TiO2 composite white pigment and preparation method thereof ", use white mineral powder is disclosed, as calcium carbonate, kaolin, calcined kaolin and barite etc. are bag core matrix, crystal TiO
2for the coating thing, in the wet ultra-fine grinding system, by grain-grain, coat modification mode, realize TiO
2at reaction coating and the modifying and decorating of bag core matrix surface, white mineral powder-TiO that preparation has pigmentary titanium dioxide character thus
2the method of composite white pigment.But the method is owing to existing, and bonding force is strong, grain-grain coats is the quality problems such as to carry out on the secondary agglomeration particle, can only in low and middle-grade products of part industry, obtain the appropriateness application, and cost is higher.
The Chinese patent application that the application number of Japan Nittetsu Mining Co., Ltd. is 01813600.1, the employing carbonating process is disclosed, prepared and a kind ofly can present the method for titanium dioxide natural characteristics as the titanium dioxide calcium carbonate composite particles of height opacity, the method is to add the TiO 2 particles with median size 0.1～0.5 μ m in carbonation step, be typically under agitation, the mixture of introducing carbon dioxide gas and air in calcium hydroxide slurry, carry out carbonation reaction, and the pH that continuation importing gaseous mixture makes reaction proceed to slurry is 7.Final acquisition relates to and contains combination above-mentioned composite particles ground composite composition wherein, can be applicable to coating and the pigment of paper grade (stock), and matrix material such as paper, plastic shaping material and rubber-moulding material etc.The method utilization has the calcium carbonate technological process of production now, can realize suitability for industrialized production after increasing the part operation, as long as composite pigment meets the use properties requirement, application prospect is very good, but the combination of the calcium carbonate of composite titanium dioxide prepared by the method and titanium dioxide is firm not, opacifying power is strong not, and weathering resistance is not high.
Summary of the invention
In view of this, the first purpose of the present invention is to provide a kind of composite titanium dioxide of with low cost, better performances, and the second purpose of the present invention is to provide a kind of method for preparing composite titanium dioxide.
In first aspect, the invention provides a kind of composite titanium dioxide, described composite titanium dioxide is by obtaining at illite surface clad nano titanium dioxide granule, prepared by the component of following ratio of weight and number by described composite titanium dioxide: 60 ~ 80 parts of illites, 15 ~ 35 parts of titanium dioxide, 0.5 ~ 5 part of dispersion agent.
Described dispersion agent is at least one in Sodium hexametaphosphate 99, water glass, trolamine, citric acid, oleic acid, sodium oleate in the present invention.
Preferably, in the present invention described illite is 1250 orders or above powder.
Preferably, in the present invention described illitic Hunter whiteness is 80 ~ 95.
Preferably, in the present invention illitic Hunter whiteness is 86 ~ 90.
A kind of method for preparing described illite based composite titanium white powder, comprise the steps:
(1) deposition: by 1250 orders or above illite, adding water, to be mixed with concentration be 100～500g/L slurries, stir and add dispersion agent, then add precipitation agent and stir, add pH adjusting agent, regulating slurry pH value is 1.0～3.0, makes the composite titanium dioxide slurries of surface deposition Nano titanium dioxide; Wherein, described precipitation agent is a kind of in titanium sulfate, titanium tetrachloride, titanyl sulfate;
(2) washing and filtering: the composite titanium dioxide slurries that deposition step is obtained wash and filter, and obtain filter cake;
(3) calcining: the filter cake after the washing that the washing and filtering step is obtained is calcined 6～10 hours under 500～800 degree, after calcining, is pulverized, and obtains the illite based composite titanium white powder.
In the preparation method of illite based composite titanium white powder, described pH adjusting agent is middle strong acid or strongly-acid material and/or alkaline matter.
Preferably, the preparation method of illite based composite titanium white powder, comprise the steps:
(1) pulp: illite is added to water and stir, being mixed with concentration is 100～500g/L slurries, adds dispersion agent, obtains slurries;
(2) wet method sand milling: the slurries that the pulp step is obtained proceed in sand mill, carry out the wet method sand milling, make 1250 orders or above illite;
(3) deposition: the illite that wet method sand milling step is made, add precipitation agent and stir, add pH adjusting agent, regulating slurry pH value is 1.0～3.0, makes the composite titanium dioxide slurries of surface deposition Nano titanium dioxide; Wherein, described precipitation agent is a kind of in titanium sulfate, titanium tetrachloride, titanyl sulfate;
(4) washing and filtering: the composite titanium dioxide slurries that deposition step is obtained wash and filter, and obtain filter cake;
(5) calcining: the filter cake after the washing that the washing and filtering step is obtained is calcined 6～10 hours under 600～800 degree, after calcining, is pulverized, and obtains the illite based composite titanium white powder.
Illite based composite titanium white powder provided by the invention has following advantage:
1, cost is low, whiteness is high;
2, strong covering power, can be used as high covering power pigment and use;
3, oil-absorption(number) is low;
4, water-soluble salt figure is low.
Embodiment
Here special-purpose word " exemplary " means " as example, embodiment or illustrative ".Here needn't be interpreted as being better than or being better than other embodiment as " exemplary " illustrated any embodiment.
In addition, for better explanation the present invention, provided numerous details in embodiment hereinafter.It will be appreciated by those skilled in the art that and there is no these details, the present invention can implement equally.In the other example, the method for knowing for everybody, means and material are not described in detail, so that highlight purport of the present invention.
Embodiment 1
Taking granularity is the illite 60g that 1250 orders, Hunter whiteness are 86, adds water 600g, is mixed with the 100g/L slurries, adds the sodium hexametaphosphate solution 15g that massfraction is 20% simultaneously, and stirs.Keep whipped state, add 100g/L titanium sulfate solution 210ml, regulating slurry pH value is 1.0, makes the composite titanium dioxide slurries of surface deposition Nano titanium dioxide.
The composite titanium dioxide slurries that deposition is obtained with the deionized water washing of pulling an oar, obtain filter cake under 40-50 ℃ of condition after filtration;
The filter cake that washing and filtering is obtained is calcined 6 hours under 700 degree, after calcining, is pulverized, and obtains the illite based composite titanium white powder.
Embodiment 2
Taking granularity is the illite 70g that 2000 orders, Hunter whiteness are 89, adds water 350g, is mixed with the 200g/L slurries, adds the sodium silicate solution 1.75g that massfraction is 20% simultaneously, and stirs.Keep whipped state, add 200g/L titanium tetrachloride solution 68ml, regulating slurry pH value is 2.0, makes the composite titanium dioxide slurries of surface deposition Nano titanium dioxide.
The composite titanium dioxide slurries that deposition is obtained with the deionized water washing of pulling an oar, obtain filter cake under 40-50 ℃ of condition after filtration;
Filter cake after the washing that washing and filtering is obtained is calcined 8 hours under 800 degree, after calcining, is pulverized, and obtains the illite based composite titanium white powder.
Embodiment 3
Taking granularity is the illite 65g that 1500 orders, Hunter whiteness are 87, adds water 130g, is mixed with the 500g/L slurries, adds the sodium hexametaphosphate solution 6.5g that massfraction is 20% simultaneously, and stirs.Keep whipped state, add 100g/L titanyl sulfate solution 220ml, regulating slurry pH value is 3.0, makes the composite titanium dioxide slurries of surface deposition Nano titanium dioxide.
The composite titanium dioxide slurries that deposition is obtained with the deionized water washing of pulling an oar, obtain filter cake under 40-50 ℃ of condition after filtration;
The filter cake that washing and filtering is obtained is calcined 10 hours under 700 degree, after calcining, is pulverized, and obtains the illite based composite titanium white powder.
Embodiment 4
Taking granularity is the illite 70g that 1500 orders, Hunter whiteness are 88, adds water 200g, is mixed with the 350g/L slurries, adds the triethanolamine solution 35g that massfraction is 20% simultaneously, and stirs.Keep whipped state, add 100g/L titanyl sulfate solution 140ml, regulating slurry pH value is 3.0, makes the composite titanium dioxide slurries of surface deposition Nano titanium dioxide.
The composite titanium dioxide slurries that deposition is obtained with the deionized water washing of pulling an oar, obtain filter cake under 40-50 ℃ of condition after filtration;
The filter cake that washing and filtering is obtained is calcined 10 hours under 600 degree, after calcining, is pulverized, and obtains the illite based composite titanium white powder.
Embodiment 5
The illite 40g that is 87 by Hunter whiteness, add water 200g, is mixed with the 200g/L slurries, adds the sodium hexametaphosphate solution 2g that massfraction is 20% simultaneously, and stir, and obtains slurries;
The slurries that pulp is obtained proceed in sand mill, carry out the wet method sand milling, make 1250 purpose illite slurries;
Keep whipped state, add 100g/L titanyl sulfate solution 100ml, regulating slurry pH value is 2.0, makes the composite titanium dioxide slurries of surface deposition Nano titanium dioxide.
The composite titanium dioxide slurries that deposition is obtained with the deionized water washing of pulling an oar, obtain filter cake under 40-50 ℃ of condition after filtration;
The filter cake that washing and filtering is obtained is calcined 8 hours under 800 degree, after calcining, is pulverized, and obtains the illite based composite titanium white powder.
About pH adjusting agent, according to the pH of slurries, select, can be middle strong acid or strongly-acid material and/or alkaline matter.Can be sulfuric acid, hydrochloric acid, oxalic acid, highly basic etc.
Comparative Examples 1
Commercially available titanium dioxide (domestic certain sulfuric acid method titanium pigment manufacturer product)
Comparative Examples 2
Commercially available composite titanium dioxide.
The performance index contrast of table 1 composite titanium dioxide of the present invention and common commercially available titanium dioxide and commercially available composite titanium dioxide
From table can draw, the whiteness of illite based composite titanium white powder of the present invention is not less than or higher than commercially available ordinary titanium powder, commercially available composite titanium dioxide.Opacifying power is better than ordinary titanium powder, suitable with commercially available composite titanium dioxide, can be used as high covering power pigment and uses.Oil-absorption(number) is lower than commercially available composite titanium dioxide.The more commercially available common white powder of water-soluble salt, commercially available composite titanium dioxide are low, have advantage in application system.
Composite titanium dioxide manufacturing cost provided by the invention is not only lower than ordinary titanium powder, also lower than existing commercially available composite titanium dioxide.Existing composite titanium dioxide, the matrix kernel adopted has light calcium carbonate, calcium carbonate, kaolin, calcined kaolin, barite etc., these matrixes have plenty of to be needed, through complex process, to have plenty of matrix and cause more greatly product particle larger, has plenty of cost higher.The present invention uses illite for the matrix kernel.Illite is a kind of new mineral of China, is common a kind of clay mineral, has rich potassium, high alumina, low iron and superior chemistry, the physicals such as smooth, bright, fine and smooth, heat-resisting.Illitic cost is very low.
Illitic whiteness own is generally not high, is 80 ~ 95, and common illite whiteness is between 85～90.The present invention, in the situation that the whiteness of matrix kernel own is not high, provides a kind of composite titanium dioxide that is equivalent to commercially available ordinary titanium powder, commercially available composite titanium dioxide whiteness, has good parameter and lower cost simultaneously.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; can expect easily changing or replacing, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion by the described protection domain with claim.
Claims (8)
1. an illite based composite titanium white powder, it is characterized in that, on the illite surface, the clad nano titanium dioxide granule obtains, and described composite titanium dioxide is made by the component of following ratio of weight and number: 60 ~ 80 parts of illites, 15 ~ 35 parts of titanium dioxide, 0.5 ~ 5 part of dispersion agent.
2. illite based composite titanium white powder according to claim 1, is characterized in that, described dispersion agent is one or more in Sodium hexametaphosphate 99, water glass, trolamine, citric acid, oleic acid, sodium oleate.
3. illite based composite titanium white powder according to claim 1, is characterized in that, described illite is 1250 orders or above powder.
4. illite based composite titanium white powder according to claim 3, is characterized in that, described illitic Hunter whiteness is 80 ~ 95.
5. according to the described illite based composite titanium white powder of claim 3 or 4, it is characterized in that, described illitic Hunter whiteness is 86 ~ 90.
6. a method for preparing illite based composite titanium white powder as described as claim 1～5 any one, is characterized in that, comprises the steps:
(1) deposition: by 1250 orders or above illite, adding water, to be mixed with concentration be 100～500g/L slurries, stir and add dispersion agent, then add precipitation agent and stir, add pH adjusting agent, regulating slurry pH value is 1.0～3.0, makes the composite titanium dioxide slurries of surface deposition Nano titanium dioxide; Wherein, described precipitation agent is a kind of in titanium sulfate, titanium tetrachloride, titanyl sulfate;
(2) washing and filtering: the composite titanium dioxide slurries that deposition step is obtained wash and filter, and obtain filter cake;
(3) calcining: the filter cake that the washing and filtering step is obtained is calcined 6～10 hours under 500～800 degree, after calcining, is pulverized, and obtains the illite based composite titanium white powder.
7. the preparation method of illite based composite titanium white powder according to claim 6, is characterized in that, described pH adjusting agent is middle strong acid or strongly-acid material and/or alkaline matter.
8. according to the preparation method of the described illite based composite titanium white powder of claim 6 or 7, it is characterized in that, comprise the steps:
(1) pulp: illite is added to water and stir, being mixed with concentration is 100～500g/L slurries, adds dispersion agent, obtains slurries;
(2) wet method sand milling: the slurries that the pulp step is obtained proceed in sand mill, carry out the wet method sand milling, make 1250 orders or above illite;
(3) deposition: the illite that wet method sand milling step is made, add precipitation agent and stir, add pH adjusting agent, regulating slurry pH value is 1.0～3.0, makes the composite titanium dioxide slurries of surface deposition Nano titanium dioxide; Wherein, described precipitation agent is a kind of in titanium sulfate, titanium tetrachloride, titanyl sulfate;
(4) washing and filtering: the composite titanium dioxide slurries that deposition step is obtained wash and filter, and obtain filter cake;
(5) calcining: the filter cake after the washing that the washing and filtering step is obtained is calcined 6～10 hours under 600～800 degree, after calcining, is pulverized, and obtains the illite based composite titanium white powder.
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| CN106082320A (en) * | 2016-06-23 | 2016-11-09 | 吉林大学 | A kind of hydrothermal synthesis method of Erie ground mass anatase complex |
| CN106189374A (en) * | 2016-07-05 | 2016-12-07 | 承德人和矿业有限责任公司 | A kind of composite granule and preparation method thereof |
| CN106280573A (en) * | 2016-08-03 | 2017-01-04 | 江苏大学 | A kind of strengthen Rutile type titanium dioxide substance whiteness and the method for brightness |
| CN109504136A (en) * | 2018-11-21 | 2019-03-22 | 延边大学 | A kind of nano-TiO2/ Erie ground mass silicon oxide composite unit interior wall coating and preparation method |
| CN110564179A (en) * | 2019-08-21 | 2019-12-13 | 中国科学院过程工程研究所 | Method for preparing composite titanium dioxide by using waste silicon slag discharged in zirconium oxychloride production |
| CN111206454A (en) * | 2020-02-10 | 2020-05-29 | 成都工业学院 | Silicon-aluminum-titanium-based composite material and preparation method and application thereof |
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| CN106280573A (en) * | 2016-08-03 | 2017-01-04 | 江苏大学 | A kind of strengthen Rutile type titanium dioxide substance whiteness and the method for brightness |
| CN106280573B (en) * | 2016-08-03 | 2018-08-07 | 江苏大学 | A method of enhancing rutile type titanium white substance whiteness and brightness |
| CN109504136A (en) * | 2018-11-21 | 2019-03-22 | 延边大学 | A kind of nano-TiO2/ Erie ground mass silicon oxide composite unit interior wall coating and preparation method |
| CN109504136B (en) * | 2018-11-21 | 2020-09-18 | 延边大学 | Nano TiO (titanium dioxide)2Interior wall coating of silica complex based on illite and preparation method thereof |
| CN110564179A (en) * | 2019-08-21 | 2019-12-13 | 中国科学院过程工程研究所 | Method for preparing composite titanium dioxide by using waste silicon slag discharged in zirconium oxychloride production |
| CN111206454A (en) * | 2020-02-10 | 2020-05-29 | 成都工业学院 | Silicon-aluminum-titanium-based composite material and preparation method and application thereof |
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Inventor after: Li Jie Inventor after: Cao Guojun Inventor after: Qu Jingkui Inventor after: Qi Tao Inventor before: Cao Guojun Inventor before: Qi Tao |
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